WO2019035104A1 - Matériau composite renforcé présentant des propriétés mécaniques et thermiques améliorées et son procédé d'obtention - Google Patents

Matériau composite renforcé présentant des propriétés mécaniques et thermiques améliorées et son procédé d'obtention Download PDF

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WO2019035104A1
WO2019035104A1 PCT/IB2018/056278 IB2018056278W WO2019035104A1 WO 2019035104 A1 WO2019035104 A1 WO 2019035104A1 IB 2018056278 W IB2018056278 W IB 2018056278W WO 2019035104 A1 WO2019035104 A1 WO 2019035104A1
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Prior art keywords
silicon
composite material
reinforced composite
polymer
silicon polymer
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PCT/IB2018/056278
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English (en)
Inventor
Eugenio Hernan OTAL
Manuela Leticia KIM
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Consejo Nacional De Investigaciones Científicas Y Técnicas (Conicet)
Iindumentaria Protectiva Rasa Sa Agencia En Chile
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Priority to US16/639,910 priority Critical patent/US20200263348A1/en
Publication of WO2019035104A1 publication Critical patent/WO2019035104A1/fr

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    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
    • C08B15/10—Crosslinking of cellulose
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
    • C08G83/001—Macromolecular compounds containing organic and inorganic sequences, e.g. organic polymers grafted onto silica
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
    • C08J3/245—Differential crosslinking of one polymer with one crosslinking type, e.g. surface crosslinking
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
    • D06M11/79—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof with silicon dioxide, silicic acids or their salts
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/0043—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by their foraminous structure; Characteristics of the foamed layer or of cellular layers
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02—Natural fibres, other than mineral fibres
    • D06M2101/04—Vegetal fibres
    • D06M2101/06—Vegetal fibres cellulosic
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/32—Polyesters
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/34—Polyamides
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/34—Polyamides
    • D06M2101/36—Aromatic polyamides
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/38—Polyurethanes
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2400/00—Specific information on the treatment or the process itself not provided in D06M23/00-D06M23/18
    • D06M2400/01—Creating covalent bondings between the treating agent and the fibre
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N2201/00—Chemical constitution of the fibres, threads or yarns
    • D06N2201/02—Synthetic macromolecular fibres
    • D06N2201/0263—Polyamide fibres
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N2201/00—Chemical constitution of the fibres, threads or yarns
    • D06N2201/02—Synthetic macromolecular fibres
    • D06N2201/0263—Polyamide fibres
    • D06N2201/0272—Aromatic polyamide fibres
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N2201/00—Chemical constitution of the fibres, threads or yarns
    • D06N2201/02—Synthetic macromolecular fibres
    • D06N2201/0281—Polyurethane fibres
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N2201/00—Chemical constitution of the fibres, threads or yarns
    • D06N2201/04—Vegetal fibres
    • D06N2201/042—Cellulose fibres, e.g. cotton
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N2209/00—Properties of the materials
    • D06N2209/06—Properties of the materials having thermal properties
    • D06N2209/065—Insulating
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/12—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins
    • D06N3/128—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins with silicon polymers

Definitions

  • the present invention relates to the field of thermally insulating materials, in particular silica aerogels and to methods of improving the mechanical properties thereof.
  • silica aerogels as thermal insulators is justified by its advantageous properties, namely low thermal conductivity, high thermal resistance and low weight as compared to ceramic materials. However, they exhibit poor mechanical properties, in particular a very low resistance to mechanical stress. This can be attributed to both their chemical structure that is close to that of glass, and their high porosity characteristics.
  • Siloxanes are the main component in silicone sealers and kitchen utensils, which are flexible and resistant to high temperatures.
  • aerogels have provided thermal insulation, flexibility, and some degree of reinforcement for use in textiles.
  • durability with intensive use, washing, and mechanical protection require a strong adhesion between the materials of the composite.
  • silicon polymers e.g., silica aerogels
  • the strategy described herein is to obtain an interphase between the textile and the silicon polymer (e.g., aerogel), in order to improve adhesion between the textile and the silicon polymer (e.g., aerogel).
  • An interphase comprises one or more covalent bonds and/or one or more hydrogen bonds between the textile and the silicon polymer (e.g., aerogel).
  • said interphase comprises
  • silanols obtained from the hydrolysis of a silicon compound such as, for example, a silicon alkoxide, silicon
  • alkylalkoxide and the like, and combinations thereof.
  • interphase comprises hydrogen bond unions between -NH 2 and/or -OH groups on a fiber surface and silanol groups.
  • R-H 2 N ⁇ ⁇ - Si bonds and R-OH ⁇ HO-Si bonds are examples of such interphase components, where R is the remainder of a fiber.
  • amino groups can be formed by hydrolysis of amide bonds of, for example, aramid or aromatic polyamide fibers.
  • a polyamide is a polyphthalamide.
  • hydroxyl groups can be formed by hydrolysis of ester bonds of, for example, polyester fibers, or are naturally-present in the textile (e.g., cotton textiles).
  • a reinforced composite material comprising: an organic polymer; a silicon polymer; and an interphase between said organic polymer and said silicon polymer, wherein said interphase comprises chemical bonds (e.g., one or more covalent bonds and/or one or more hydrogen bonds) between the organic polymer and the silicon polymer.
  • the organic polymer is a textile material.
  • the textile material is selected from the group consisting of cotton, polyamide fibers (e.g., aramid fibers), polyester fibers, polyurethane fibers, and the like, and combinations thereof.
  • the textile material comprises/is a polyamide fiber (e.g., aliphatic, semi-aromatic, fully aromatic polyamides or a combination thereof) and the chemical bonds between the organic polymer and the silicon polymer comprise R-H 2 N ⁇ HO-Si hydrogen bonds and/or R-OH ⁇ HO-Si bonds, where R is remainder of the polymer, between the surface - H 2 or -OH groups of the fibers and the Si-OH groups of the silicon polymer.
  • polyamide fibers include nylons and the like.
  • Other non-limiting examples of aromatic polyamides include Nomex, Kevlar (Dupont), Technora, Heracron, Twaron, and the like.
  • the textile material comprises/is cotton and the chemical bonds between the organic polymer and the silicon polymer comprises C-O-Si covalent bonds between the cellulose of the cotton fibers and the Si-OH groups of the silicon polymer.
  • the textile material comprises/is a polyurethane, polyester, or polyamide fiber the chemical bonds between the organic polymer and the silicon polymer comprise R-H 2 N ⁇ ⁇ -Si or
  • R-OH- ⁇ ⁇ -Si hydrogen bonds where R is remainder of the polyamide, polyester or polyurethane polymer, between the hydrolyzed -NH 2 or -OH groups of the fiber(s) and the Si-OH groups of the silicon polymer.
  • the silicon polymer is a silica aerogel. It is another object of the present invention to provide a method to obtain a reinforced composite material, comprising:
  • the organic polymer is a textile fabric and the step of obtaining an interphase between said organic polymer and said silicon polymer further comprises contacting (e.g., washing) said textile fabric with a mixture comprising a basic compound (e.g., metal hydroxides, such as, for example, sodium hydroxide, potassium hydroxide, and the like, tetramethylammonium hydroxide, DABCO, and the like) and contacting (e.g., pretreating) said fabric with a mixture comprising a silicon compound.
  • a basic compound e.g., metal hydroxides, such as, for example, sodium hydroxide, potassium hydroxide, and the like, tetramethylammonium hydroxide, DABCO, and the like
  • the basic compound(s) provide/provides a mixture (e.g., a solution in water) having a pH of 8-14, including all 0.1 pH values and ranges therebetween.
  • the basic compound(s) provide/provides a mixture (e.g., a solution in or comprising water) having a pH of at least 8, at least 8.5, at least 9, at least 9.5, at least 10, at least 10.5.
  • the basic compound(s) provide/provides a mixture (e.g., a solution in or comprising water) having a pH of at least 8, at least 8.5, at least 9, at least 9.5, at least 10, at least 10.5 at a temperature of about room temperature (e.g., 18-25 °C) to about 200 °C, including all integer °C values and ranges therebetween.
  • a mixture e.g., a solution in or comprising water having a pH of at least 8, at least 8.5, at least 9, at least 9.5, at least 10, at least 10.5 at a temperature of about room temperature (e.g., 18-25 °C) to about 200 °C, including all integer °C values and ranges therebetween.
  • the methods are carried out at (e.g., in a mixture having a) pH of 8-14, including all 0.1 pH values and ranges therebetween.
  • the methods are carried out at (e.g., in a mixture having a) pH of at least 8, at least 8.5, at least 9, at least 9.5, at least 10, at least 10.5.
  • the methods are carried out at (e.g., in a mixture having a) at least 8, at least 8.5, at least 9, at least 9.5, at least 10, at least 10.5 at a temperature of a temperature of about room temperature (e.g., 18-25 °C) to about 200 °C, including all integer °C values and ranges therebetween.
  • the mixture may comprise a basic compound and one or more solvents.
  • the solvent comprises/is water.
  • the solvent comprises water and/or one or more alcohols.
  • the time, concentration of basic compound(s), and temperature of the contacting are correlated. For example, higher temperature and/or concentration generally means shorter times.
  • contacting (e.g., washing) the textile with the mixture comprising a basic compound provides only surface - H 2 and/or -OH groups and does not degrade the fiber.
  • the contacting (e.g., washing) the textile with the mixture comprising a basic compound provides only surface - H 2 and/or -OH groups.
  • contacting e.g., washing
  • the textile does not substantially affect one or more mechanical property of the textile.
  • one or more of the mechanical properties of the textile after being contacted with the mixture comprising a basic compound is the same or substantially the same (e.g., changed by 5% or less, 4% or less, 3% or less, 2% or less, 1% or less) compared to same mechanical property(ies) of the a textile having the same composition (e.g., the same textile) that has not been being contacted with the mixture.
  • the organic polymer is a polyamide fiber.
  • polyamides include, but are not limited to, aliphatic, aromatic, and semi-aromatic polyamides and combinations thereof.
  • Non-limiting examples of polyamides include nylon materials.
  • Aramids are examples of aromatic polyamides.
  • the organic polymer is an aramid fiber.
  • the organic polymer is a polyurethane fiber.
  • the organic polymer is a polyester fiber.
  • the organic polymer is a polyamide fiber.
  • the organic polymer is a cotton fiber.
  • the basic compound is sodium hydroxide and the silicon compound is a silicon alkoxide.
  • the silicon alkoxide may be a partially alkylated silicon alkoxide.
  • the number of carbons in the alkyl portion of the alkoxide being, independently, for example, 1, 2, 3, 4, 5, or any the amount that can be partially hydrolyzed.
  • the silicon alkoxide e.g., partially hydrolyzed silicon alkoxide
  • the silicon alkoxide is tetraethyl orthosilicate and/or tetramethyl orthosilicate.
  • the silicon-containing compound is a silicate (e.g., sodium silicate).
  • the step of obtaining silicon polymer from the silicon polymer precursor comprises polymerizing the silicon polymer precursor.
  • the step of polymerizing the silicon polymer precursor comprises steps of hydrolysis of the silicon polymer precursor, condensation, and thermal treatment (e.g., heating, such as, for example, curing).
  • the method further includes a step of drying.
  • the method is carried out at a temperature of about room temperature (e.g., 18-25 °C) to about 200 °C, including all integer °C values and ranges therebetween.
  • the silicon polymer precursor comprises an alkyltrialkoxysilane
  • dialkyldialkoxysilane trialkylalkoxysilane, or a combination thereof.
  • the number of carbons in the alkyl group and/or alkyl portion of the alkoxide (R) being, independently, for example, 1, 2, 3, 4, 5, or any the amount that can be partially hydrolyzed.
  • the partially hydrolyzed alkyltrialkoxysilane does not precipitate before the application on the textile and/or can form a covalent of hydrogen bond with the pre- hydrolyzed fibers.
  • the alkyltrialkoxisilane is methyltriethoxysilane.
  • the alkyl group in a tetraalkoxysilane or alkyltrialkoxysilane plays a role of improving the hydrogen bonds formed by and van der Waals interactions of the
  • alkyltrialkoxysilane The length of the alkyl group and alkyl portion of the alkoxy groups effect the relative hydrolysis rate and condensation rate of the tetraalkoxysilane or alkyltrialkoxysilane.
  • Figure 1 shows the Fourier transform infrared spectroscopy (FTIR) spectrum of the untreated aramid fiber sample.
  • Figure 2 shows the ratio of FTIR spectrum bands corresponding to the aliphatic chain (823 cm “1 ) and the amides (1647 cm “1 ) of aramid fiber samples.
  • Figure 3 shows the results of transversal traction tests carried out on aramid fiber samples prepared with different surface preparation treatments as described herein.
  • Figure 4 shows the results of longitudinal traction tests carried out on aramid fiber samples prepared with different surface preparation treatments.
  • Figure 5 shows examples of polyamide hydrolysis, polyester hydrolysis, and polyurethane hydrolysis.
  • sica aerogel refers to a non-fluid ultralight silica polymer network dispersed in a gas such as air.
  • a gas such as air.
  • silica alcogel When the polymerized precursor of silica is gelified in an alcoholic solvent, such as methanol or ethanol, the term “silica alcogel” is usually employed.
  • silicon precursor or "silicon polymer precursor” refers to a compound from which a silicon polymer can be obtained.
  • textile or “textile material” refers to a flexible material consisting of a network of woven or unwoven, natural or synthetic fibers.
  • the term "reinforced” refers to material with one or more enhanced properties (e.g., increased physical properties, increased thermal resistance, enhanced adhesion between materials in a composite, etc.)
  • the inventors were able to generate an interphase between the textile and the aerogel.
  • Said interphase comprises silanol groups which are chemically bonded to the textile, by means of covalent bonds in the case of cotton and hydrogen bonds in the case of polyamides (e.g., aramids), and that allows the growth of a silica aerogel on said interphase, where the aerogel comprises Si-O-Si covalent bonds.
  • the generated interphase acts as an intermediary that allows the bonding of an organic polymer (e.g., natural or synthetic or a combination thereof) with a silicon polymer (e.g., an aerogel).
  • an organic polymer e.g., natural or synthetic or a combination thereof
  • a silicon polymer e.g., an aerogel
  • the obtained composite materials have a global structure, for example, given by (textile // surface groups in the textile from the hydrolysis process // surface silanol groups // aerogel), which confers the material the ability to withstand undesirable (e.g., severe) conditions and the possibility to be washed in order to remove pollutants, without a decrease in the thermal insulation properties.
  • the silicon polymer e.g., aerogel
  • the silicon polymer can be formed using various silicon compounds. Mixtures of silicon compounds can be used.
  • the silicon compound is a silicon alkoxide (e.g., a tetraalkoysilane).
  • the silicon alkoxide may be a partially or completely alkylated silicon alkoxide.
  • the number of carbons in the alkyl portion of the alkoxide group being, for example, 1, 2, 3, 4, 5, or any the amount that can be partially hydrolyzed.
  • the silicon alkoxide e.g., partially hydrolyzed silicon alkoxide does not precipitate before the application on the textile and/or can form a covalent of hydrogen bond with the pre-hydrolyzed fibers.
  • the silicon alkoxide is tetraethyl orthosilicate and/or tetramethyl orthosilicate.
  • the silicon-containing compound is a silicate (e.g., sodium silicate).
  • silicon polymer e.g., aerogel
  • a thickness e.g., a dimension perpendicular to a surface of a fiber
  • the silicon polymer may be a continuous or discontinuous layer disposed on a fiber surface.
  • the steps of the method described in the various embodiments and examples disclosed herein are sufficient to carry out the method of the present disclosure.
  • the method consists essentially of a combination of the steps of the method disclosed herein.
  • the method consists of such steps.
  • a washing solution was prepared by dissolving 5.0 g of NaOH in 20 mL of water. 1.5 g of Triton X-100 and 0.75 g of citric acid were added and the solution was completed with water to 500 mL.
  • the washed samples were immersed in a 2% tetraethyl orthosilicate (TEOS) in an ethanol/water 80:20 mixture.
  • TEOS tetraethyl orthosilicate
  • silica alcogels were prepared via precursor hydrolysis and condensation, curing and subsequent drying at ambient pressure. Typically, the molar relation
  • MTES methyltriethoxysilane
  • methanol:oxalic acid 0.001 mol/L
  • NH 3 10 mol/L
  • Precursor hydrolysis 4 mL of MTES were mixed with 22.4 mL of methanol
  • wet gels were dried at atmospheric pressure in a three-stage furnace, at 50 °C for 12 h, 80 °C for 2 h and finally at 200 °C for 2 h.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Dispersion Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Materials Engineering (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Reinforced Plastic Materials (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)

Abstract

La présente invention concerne un matériau composite renforcé, comprenant un polymère organique, un polymère de silicium et une interphase entre ledit polymère organique et ledit polymère de silicium, ladite interphase comprenant des liaisons chimiques entre le polymère organique et le polymère de silicium, et un procédé pour obtenir ledit matériau composite renforcé. La présente invention peut être utilisée pour améliorer les propriétés mécaniques d'aérogels de silice par la fonctionnalisation de matériaux textiles.
PCT/IB2018/056278 2017-08-18 2018-08-20 Matériau composite renforcé présentant des propriétés mécaniques et thermiques améliorées et son procédé d'obtention WO2019035104A1 (fr)

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